CN112142876B - Method for coagulating butadiene rubber solution - Google Patents
Method for coagulating butadiene rubber solution Download PDFInfo
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- CN112142876B CN112142876B CN201910569408.3A CN201910569408A CN112142876B CN 112142876 B CN112142876 B CN 112142876B CN 201910569408 A CN201910569408 A CN 201910569408A CN 112142876 B CN112142876 B CN 112142876B
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- C08C—TREATMENT OR CHEMICAL MODIFICATION OF RUBBERS
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Abstract
The invention relates to the field of rubber product preparation, and discloses a method for coagulating butadiene rubber solution, which comprises the following steps: mixing part of the post-treatment circulating hot water A with a butadiene rubber solution to obtain a heterogeneous mixture, and sequentially feeding the heterogeneous mixture into a first condensation kettle, a second condensation kettle and a third condensation kettle to remove a solvent; and carrying out first heat exchange on the other part of the post-treatment circulating hot water B and steam to obtain superheated water and first steam condensate water, and feeding the superheated water into a second condensation kettle from the bottom of the second condensation kettle. The method can improve the heat utilization efficiency of the device and reduce the discharged sewage quantity of the device.
Description
Technical Field
The invention relates to the field of rubber product preparation, in particular to a method for coagulating butadiene rubber solution.
Background
The solvent removing process of the solution polymerization synthesis device adopts a multi-kettle series connection elutriation method coagulation process based on the steam distillation and wet degassing. In the traditional process design, the heat supply mode of the process is that steam is directly used for supplying heat, the process is simple, the heat utilization efficiency is high, but the process has the problem that in order to balance the material inlet and outlet, oily sewage with the same amount as the steam inlet amount must be discharged out of a system, and the process has increasingly embodied limitations at present when the pollution discharge amount and the standard of a chemical production device are increasingly strict.
Disclosure of Invention
The invention aims to improve the sewage discharge of the device, and provides heat required by partial steam stripping by heating circulating hot water to an overheated state and introducing the superheated circulating hot water into a steam stripping kettle in a way of changing the heat supply mode in the condensation process on the premise of not changing the process conditions of the original steam stripping kettle. The method can reduce the amount of sewage discharged by the device, and the steam condensate with higher enthalpy can be fully reused, thereby improving the heat utilization efficiency of the device.
In order to achieve the above object, the present invention provides a method for coagulating a butadiene rubber solution, the method comprising: mixing part of the post-treatment circulating hot water A with a butadiene rubber solution to obtain a heterogeneous mixture, and sequentially feeding the heterogeneous mixture into a first condensation kettle, a second condensation kettle and a third condensation kettle to remove a solvent; and carrying out first heat exchange on the other part of the post-treatment circulating hot water B and steam to obtain superheated water and first steam condensate water, and feeding the superheated water into a second condensation kettle from the bottom of the second condensation kettle.
Preferably, a three pot differential pressure agglomeration process is employed.
Preferably, the weight ratio of the butadiene rubber contained in the butadiene rubber solution to the sum of the post-treatment circulating hot water a and B is from 0.025 to 0.075: 1.
preferably, the weight ratio of the post-treatment circulating hot water B to the post-treatment circulating hot water A is 0.15-0.4: 1.
preferably, before part of the post-treatment circulating hot water A is mixed with the butadiene rubber solution, the first steam condensate and the butadiene rubber solution are subjected to second heat exchange, so that the first steam condensate is further cooled to obtain second steam condensate.
Preferably, the steam temperature is 125-200 ℃.
Preferably, the superheated water temperature is 125-145 ℃.
Preferably, the temperature of the first steam condensate water is 140-200 ℃, the pressure is 0.4-0.8MPa, the temperature of the second steam condensate water is 85-125 ℃, and the pressure is 0.4-0.8 MPa.
Preferably, the gas phase at the top outlets of the second condensation kettle and the third condensation kettle enters the bottom of the first condensation kettle, and the solvent gas phase is evaporated from the top of the first condensation kettle, passes through a stripping gas filter and a condensing cooler and then enters the oil-water layering tank for layering.
Preferably, the butadiene rubber solution is a butadiene rubber solution.
Preferably, the operating pressure of the first coagulation-up kettle is 0.01-0.03MPa, and the temperature is 80-90 ℃.
Preferably, the operating pressure of the second condensation kettle is 0.06-0.1MPa, and the temperature is 100-120 ℃.
Preferably, the third coagulation-up kettle is operated at a pressure of 0.004-0.006MPa and a temperature of 95-115 ℃.
In the traditional multi-kettle condensation process, steam directly enters a condensation kettle to provide heat and then becomes steam condensate water to enter a post-treatment process along with colloidal water particles, hot water is recycled and then returns to the condensation process for recycling (namely post-treatment circulating hot water), and in order to balance the circulating hot water amount, the circulating hot water changed from the steam becomes sewage after deducting the hot water loss amount of the post-treatment process and is discharged outside; by the method provided by the invention, steam does not directly enter the condensation kettle, but exchanges heat with part of circulating hot water to change the circulating hot water into superheated water to enter the condensation kettle, so that the condensation effect of the condensation kettle is ensured, the external discharge of sewage is reduced, the environmental protection requirement is met, and the subsequent sewage treatment cost is reduced.
Drawings
FIG. 1 is a flow chart of a three-pot differential pressure coagulation process for a dope in example 1.
FIG. 2 is a flow chart of a three-pot differential pressure coagulation process of a prior art cement in comparative example 1.
Description of the reference numerals
R-1: a first coagulation vessel; r-2: a second coagulation vessel; r-3: a third coagulation kettle; p-1: a first coagulation kettle water colloidal particle pump; p-2: a second coagulation kettle water colloidal particle pump; p-3: a third coagulation kettle water colloidal particle pump; x-1: a first coalescer stripper gas filter; x-2: a second coagulation reactor stripping gas filter; x-3: a third coagulation reactor stripping gas filter; x-4: an ejector; x-5: a water-glue mixer; e-1: a circulating hot water heater; e-2: a glue solution heater; PS: a butadiene rubber solution; HW: circulating hot water; HW-A: circulating hot water A; HW-B: circulating hot water B; LS: steam; LC: steam condensate water; WS: gas phase at the top of the kettle; WR: colloidal particle water.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
In the present invention, the term "pressure" refers to gauge pressure.
The invention provides a method for coagulating butadiene rubber solution, wherein the method comprises the following steps: mixing part of the post-treatment circulating hot water A with a butadiene rubber solution to obtain a heterogeneous mixture, and sequentially feeding the heterogeneous mixture into a first condensation kettle, a second condensation kettle and a third condensation kettle to remove a solvent; and carrying out first heat exchange on the other part of the post-treatment circulating hot water B and steam to obtain superheated water and first steam condensate water, and feeding the superheated water into a second condensation kettle from the bottom of the second condensation kettle.
According to the present invention, the method of mixing the partial post-treatment circulating hot water a with the butadiene rubber solution is not particularly limited as long as sufficient mixing is possible, and for example, the partial post-treatment circulating hot water a and the butadiene rubber solution may be mixed by introducing them into a mixer. As such a mixer, for example, an SX type mixer can be used.
In the present invention, in view of the particle diameter and size of the butadiene rubber, it is preferable that the weight ratio of the butadiene rubber contained in the butadiene rubber solution to the total amount of the post-treatment circulating hot water a and B is from 0.025 to 0.075: 1, more preferably 0.03 to 0.06: 1.
specific examples of the weight ratio of the butadiene rubber contained in the butadiene rubber solution to the total amount of the post-treatment circulating hot water a and B include, for example, 0.025: 1. 0.03: 1. 0.035: 1. 0.04: 1. 0.045: 1. 0.05: 1. 0.055: 1. 0.06: 1. 0.065: 1. 0.07: 1 or 0.075: 1, etc.
According to the present invention, the heterogeneous mixture may be fed into the first coagulation vessel by various feeding methods generally employed in the art, and preferably, the heterogeneous mixture is fed into the first coagulation vessel through a nozzle.
In the invention, steam does not directly enter the second condensation kettle, but exchanges heat with part of the post-treatment circulating hot water to change the post-treatment circulating hot water into superheated water to enter the second condensation kettle, so that the condensation effect of the second condensation kettle can be ensured, the external discharge of sewage is reduced, the environmental protection requirement is met, and the subsequent sewage treatment cost is reduced.
Preferably, the steam temperature is 125-200 ℃.
Preferably, the superheated water temperature is 125-145 ℃; more preferably, the superheated water temperature is 130-.
Preferably, the first steam condensate water temperature is 140-200 ℃, and the pressure is 0.4-0.8 Mpa; more preferably, the first steam condensate water temperature is 140-160 ℃, and the pressure is 0.4-0.8 MPa.
Preferably, the temperature of the second steam condensate water is 85-125 ℃, and the pressure is 0.4-0.8 Mpa; more preferably, the second steam condensate temperature is 95-105 ℃ and the pressure is 0.4-0.8 Mpa.
According to the invention, the steam is converted into a first steam condensate after a first heat exchange with the post-treatment circulating hot water B, the first steam condensate also has a high temperature, and the heat of the first steam condensate can be further recovered. Therefore, before part of the post-treatment circulating hot water A is mixed with the butadiene rubber solution, the first steam condensate and the butadiene rubber solution are subjected to second heat exchange, so that the first steam condensate is further cooled to obtain second steam condensate.
The first steam condensate water and the butadiene rubber solution are subjected to second heat exchange to form the second steam condensate water, so that the temperature of the butadiene rubber solution can be increased while the temperature of the butadiene rubber solution is reduced, and the condensation effect of the first condensation kettle is improved.
The first heat exchange and the second heat exchange may be performed by using various heat exchangers generally used in the art, and for example, a shell-and-tube heat exchanger may be used.
In view of controlling the particle diameter and size of the butadiene rubber, it is preferable that the weight ratio of the post-treatment circulating hot water B to the post-treatment circulating hot water a is 0.15 to 0.4: 1; more preferably, the weight ratio of the post-treatment circulating hot water B to the post-treatment circulating hot water a is 0.15 to 0.3: 1; further preferably, the weight ratio of the post-treatment circulating hot water B to the post-treatment circulating hot water a is 0.2 to 0.3: 1.
according to the invention, preferably, the outlet gas phases at the top parts of the second condensation kettle and the third condensation kettle enter the bottom part of the first condensation kettle, and the solvent gas phase is evaporated out from the top part of the first condensation kettle, passes through a stripping gas filter and a condensing cooler and then enters the oil-water separation tank for layering; more preferably, the gas phase at the outlet of the top of the second coagulation kettle directly enters the bottom of the first coagulation kettle, the gas phase at the outlet of the top of the third coagulation kettle enters the bottom of the first coagulation kettle along with steam sprayed by the steam sprayer, and the solvent gas phase is finally evaporated from the top of the first coagulation kettle and enters the oil-water separation tank for separation after passing through the stripping gas filter and the condensing cooler.
According to the invention, the butadiene rubber solution coagulation method is carried out by adopting a three-kettle differential pressure coagulation process.
According to the present invention, the operating conditions of the first coagulation-up tank may be various conditions generally used in the art, and preferably, the operating pressure of the first coagulation-up tank is 0.01 to 0.03MPa and the temperature is 80 to 90 ℃.
According to the present invention, the operating conditions of the second coagulation-up vessel may be various conditions commonly used in the art, and preferably, the operating pressure of the second coagulation-up vessel is 0.06-0.1MPa and the temperature is 100-120 ℃.
According to the present invention, the operating conditions of the third coagulation vessel may be various conditions commonly used in the art, and preferably, the operating pressure of the third coagulation vessel is 0.004 to 0.006MPa and the temperature is 95 to 115 ℃.
According to the present invention, preferably, the method further comprises introducing steam into the bottom of the first coagulation reactor for adjusting the temperature of the first coagulation reactor. That is, the temperature compensation means for the first coagulation-flocculation vessel is not a continuous means of introducing steam into the bottom of the first coagulation-flocculation vessel, but a small amount of steam is introduced to return the first coagulation-flocculation vessel to the above range when the first coagulation-flocculation vessel temperature decreases due to heat loss.
According to the present invention, preferably, the method further comprises introducing steam into the bottom of the second coagulation vessel for adjusting the temperature of the second coagulation vessel. That is, the temperature compensation means for the second coagulation-flocculation vessel is not a continuous means of introducing steam into the bottom of the second coagulation-flocculation vessel, but a small amount of steam is introduced to return the temperature of the second coagulation-flocculation vessel to the above range when the temperature of the second coagulation-flocculation vessel decreases due to heat loss.
According to the present invention, the butadiene rubber solution may be synthesized using a method generally used in the art.
Preferably, the butadiene rubber solution is a butadiene rubber solution.
According to the invention, the concentration of butadiene rubber in the butadiene rubber solution may be 12 to 25 wt.%, more preferably 13 to 15 wt.%, particularly preferably 15 wt.%.
Further, the solvent in the butadiene rubber solution is preferably one or more of cyclohexane, hexane, pentane, heptane, and octane.
The present invention will be described in detail below by way of examples, but the present invention is not limited to the following examples.
Example 1
The condensation process of this embodiment adopts a pressure difference type, and the process flow diagram is shown in fig. 1, butadiene rubber solution PS (butadiene rubber solution, solvent is cyclohexane, hereinafter referred to as glue solution) is sent to a glue solution heater E-2 to perform second heat exchange with first steam condensate, then sent to a water-glue mixer X-5 to be mixed with fed post-treatment circulating hot water a to obtain a heterogeneous mixture, the obtained heterogeneous mixture is sent to a first condensation kettle R-1, and a kettle top gas phase WS passes through a first condensation kettle stripping gas filter X-1 and a condensation cooler and then enters an oil-water layer tank for layering; in addition, feeding the post-treatment circulating hot water B into a circulating hot water heater E-1 to perform first heat exchange with fed partial steam LS to obtain first steam condensate water and superheated water, and feeding the superheated water into a second condensation kettle R-2 from the bottom of the second condensation kettle R-2; sending the colloidal particle water WR at the bottom of the first coagulation reactor R-1 into the second coagulation reactor R-2 by the first coagulation reactor colloidal particle pump P-1, sending the colloidal particle water WR at the bottom of the second coagulation reactor R-2 into the third coagulation reactor R-3 by the second coagulation reactor colloidal particle pump P-2, directly sending the gas phase WS at the top of the second coagulation reactor R-2 into the bottom of the first coagulation reactor R-1, sending the gas phase WS at the top of the third coagulation reactor R-3 into the bottom of the first coagulation reactor R-1 along with the steam sprayed by the steam sprayer X-4, finally steaming out the solvent gas phase from the top of the first coagulation reactor R-1, and sending the solvent gas phase WS to the oil-water layering tank for layering after passing through the steam stripping gas filter X-1 and the condensation cooler. And (2) sending the colloidal particle water WR at the bottom of the third coagulation kettle R-3 to a post-treatment working section through a third coagulation kettle colloidal particle pump P-3 for dehydration, drying and packaging, and in addition, in the running process, when the temperatures of the first coagulation kettle R-1 and the second coagulation kettle R-2 are lower than the preset temperature, respectively sending a small amount of steam LS from the bottom of the first coagulation kettle R-1 and the bottom of the second coagulation kettle R-2 for regulating the temperatures of the first coagulation kettle R-1 and the second coagulation kettle R-2 (namely, taking temperature compensation measures for the first coagulation kettle R-1 and the second coagulation kettle R-2).
Wherein, the three-kettle condensation process conditions are as follows: the top pressure of the first coagulation reactor is 0.02MPa, the top pressure of the second coagulation reactor is 0.08MPa, and the top pressure of the third coagulation reactor is 0.005 MPa; the temperature of the bottom of the first coagulation kettle is 89 ℃, the temperature of the bottom of the second coagulation kettle is 105 ℃, and the temperature of the bottom of the third coagulation kettle is 101 ℃; the temperature of the glue solution is 80 ℃; circulating hot water of 97 ℃; the steam temperature is 200 ℃, and the pressure is 0.45 MPa; the temperature of the first steam condensate water is 161 ℃, and the pressure is 0.45MPa, and the temperature of the second steam condensate water is 96 ℃, and the pressure is 0.44 MPa. The circulating hot water B/A is 0.2 (weight ratio); the concentration of the glue solution is 15 wt%, and the weight ratio of the rubber contained in the glue solution to the sum of the post-treatment circulating hot water A and the post-treatment circulating hot water B is 0.03: 1.
the results are shown in Table 1.
Example 2
The B/A ratio of the circulating hot water is 0.15, the other process conditions are the same as example 1, and the experimental results are shown in Table 1.
Example 3
The B/A ratio of the circulating hot water is 0.3, other process conditions are the same as example 1, and the experimental results are shown in Table 1.
Comparative example 1
The process flow diagram is shown in fig. 2, all the post-treatment circulating hot water A and B are mixed with the butadiene rubber solution and enter a first condensation kettle R-1, the steam which exchanges heat with the post-treatment circulating hot water B directly enters a second condensation kettle R-2, other process conditions are the same as those in example 1, and the experimental results are shown in table 1.
TABLE 1
Note 1: in actual production, the physical properties of the condensed glue solution of each batch in a production cycle are slightly different, so that the data in the table fluctuates within a certain range, and the values given in the table are all mean values in a production cycle.
Note 2: in the production, the third condensation kettle does not take temperature compensation measures, namely, steam is not generally introduced.
Note 3: in the production, after the steam enters the condensation process, except that a part of the steam is used as the supplement of the consumption of the circulating hot water in the post-treatment process, other steam is finally changed into sewage and is discharged to a sewage treatment system.
Note 4: the total amount of steam introduced into the three condensation kettles (the steam amount of the first kettle, the steam amount of the second kettle and the steam amount of the ejector) is the circulating hot water consumption amount and the sewage discharge amount of the post-treatment procedure
Note 5: various cost calculation bases in implementation effects are as follows: steam is 350 yuan/ton; 17 yuan/ton of condensed water; the sewage treatment cost is 7 yuan/ton.
As can be seen from table 1, in example 1 compared to comparative example 1, the steam is not directly fed into the second coagulation vessel, i.e.: the steam consumption is increased by 0.3t/h, namely the steam consumption per ton of product is increased by 0.09 ton of steam, and the cost is increased by 24.7 yuan per ton (product); the discharged sewage is reduced by 6.2t/h and 70%, and the cost is saved by 10.2 yuan/ton (product); the steam condensed water can be utilized to increase by 6.5t/h, the cost is saved by 26.0 yuan/ton (product), the total cost is saved by 11.5 yuan/ton (product), and the cost is saved by 34.5 yuan/year according to 3 ten thousand tons/year. (slightly increased steam dosage, neglected operating costs)
Social benefits are as follows: calculated according to 3 ten thousand tons of annual output, the sewage discharge is reduced by 4.3 ten thousand tons per year.
Compared with the comparative example 1, the effect of the examples 2 and 3 is the same as that of the example 1, the change of the B/A value of the circulating hot water has certain influence on the temperature of the second condensation kettle, but the temperature of the second condensation kettle fluctuates in a smaller range through the adjustment of the heat exchanger.
The agglomeration method of the present invention can be seen from the comparison of examples and comparative examples, and its significant effects include:
1. on the premise that all indexes of the product are qualified, the total steam consumption is not increased or slightly increased, a large amount of reusable steam condensate is obtained, the cost is saved, and the economic benefit is increased.
2. The sewage discharge amount is obviously reduced, and the social benefit is obtained while the economic benefit is increased.
3. High-temperature sewage can not directly enter a sewage treatment plant, and needs to be subjected to cooling pretreatment, so that the sewage discharge amount is reduced, and the cooling water consumption amount can be reduced.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (11)
1. A method of coagulating a butadiene rubber solution, the method comprising: mixing part of the post-treatment circulating hot water A with a butadiene rubber solution to obtain a heterogeneous mixture, and sequentially feeding the heterogeneous mixture into a first condensation kettle, a second condensation kettle and a third condensation kettle to remove a solvent; and before part of the post-treatment circulating hot water A is mixed with the butadiene rubber solution, the first steam condensate water and the butadiene rubber solution are subjected to second heat exchange, so that the first steam condensate water is further cooled to obtain second steam condensate water, and the temperature of the superheated water is 125-145 ℃.
2. The method of claim 1, wherein a three-pot differential pressure agglomeration process is employed.
3. The process according to claim 1, wherein the weight ratio of butadiene rubber contained in the butadiene rubber solution to the sum of the post-treatment recycled hot water A and B is from 0.025 to 0.075: 1.
4. a method according to any one of claims 1-3, wherein the weight ratio of the post-treatment recycled hot water B to the post-treatment recycled hot water a is 0.15-0.4: 1.
5. the method as claimed in any one of claims 1 to 3, wherein the steam temperature is 125-200 ℃.
6. The method as claimed in claim 5, wherein the first steam condensate temperature is 140-200 ℃ and the pressure is 0.4-0.8MPa, and the second steam condensate temperature is 85-125 ℃ and the pressure is 0.4-0.8 MPa.
7. The method according to any one of claims 1 to 3, wherein the outlet gaseous phase at the top of the second coagulation vessel and the outlet gaseous phase at the top of the third coagulation vessel enter the bottom of the first coagulation vessel, and the solvent gaseous phase is distilled out from the top of the first coagulation vessel, passes through a stripping gas filter and a condensing cooler, and then enters the oil-water separation layer tank for separation.
8. The method according to any one of claims 1 to 3, wherein the butadiene rubber solution is a butadiene rubber solution.
9. A process according to any one of claims 1 to 3, wherein the operating pressure of the first coagulation vessel is in the range of from 0.01 to 0.03MPa and the temperature is in the range of from 80 to 90 ℃.
10. The process as claimed in any one of claims 1 to 3, wherein the operating pressure of the second coagulation vessel is from 0.06 to 0.1MPa and the temperature is from 100 ℃ to 120 ℃.
11. A process according to any one of claims 1 to 3, wherein the third coagulation vessel is operated at a pressure of from 0.004 to 0.006MPa and a temperature of from 95 to 115 ℃.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3842052A (en) * | 1969-10-16 | 1974-10-15 | Snam Progetti | Process for removing the solvent from solutions of gummy polymers |
| CN101235105A (en) * | 2007-12-30 | 2008-08-06 | 中国石油大庆石油化工总厂 | Method for agglomerating solution-polymerized rubber |
| CN102516419A (en) * | 2011-12-08 | 2012-06-27 | 茂名鲁华化工有限公司 | Three-kettle condensation method used in solution polymerization production of synthetic rubber |
| CN202450017U (en) * | 2012-02-20 | 2012-09-26 | 山东齐鲁石化工程有限公司 | Three-kettle condensation device for producing synthetic rubber by using solution method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| IT1391942B1 (en) * | 2008-11-14 | 2012-02-02 | Polimeri Europa Spa | PROCEDURE FOR OBTAINING AN ELASTOMER IN THE SOLID STAGE STARTING FROM ITS POLYMERIC SOLUTION |
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- 2019-06-27 CN CN201910569408.3A patent/CN112142876B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3842052A (en) * | 1969-10-16 | 1974-10-15 | Snam Progetti | Process for removing the solvent from solutions of gummy polymers |
| CN101235105A (en) * | 2007-12-30 | 2008-08-06 | 中国石油大庆石油化工总厂 | Method for agglomerating solution-polymerized rubber |
| CN102516419A (en) * | 2011-12-08 | 2012-06-27 | 茂名鲁华化工有限公司 | Three-kettle condensation method used in solution polymerization production of synthetic rubber |
| CN202450017U (en) * | 2012-02-20 | 2012-09-26 | 山东齐鲁石化工程有限公司 | Three-kettle condensation device for producing synthetic rubber by using solution method |
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